Studies on organophosphorus compounds—V: Pyridines from secondary car☐amides and HMPA

A new pyridine synthesis has been found by refluxing certain simple secondary car☐amides in HMPA. Thus 2,6-dimethylpyridine, 2-ethyl-6-methylpyridine, 2,3,6-trimethylpyridine, 2-ethyl-3,6-dimethylpyridine, 2-benzyl-6-methyl-3-phenylpyridine, 2-ethyl-3-methyl-5,6,7,8-tetrahydroquinoline and 2-t-butyl-6-methylpyridine were prepared in 15–40% yield.     

Retention of analgin and anesthesin on sorbents with different polarities: The analysis of bellalgin tablets by high-performance liquid chromatography

The effects of acetonitrile and potassium dihydrogen phosphate concentrations in a mobile phase and the pH of the mobile phase on the retention of analgin (dipyrone) and anesthesin (benzocaine) on Symmetry C18 and Nova-Pak CN HP sorbents with grafted octadecylsilanol and nitrile groups, respectively, were studied. It was found that, under identical conditions, retention on the sorbent with grafted nitrile groups was weaker. A rapid and cost-effective procedure was developed for the determination of analgin and anesthesin in the analysis of Bellalgin tablets.     

Structure,tautomerism, and transformations of β-(3-nitro-2-pyridyl)- and β-(3-nitro-4-pyridyl)pyruvic acid esters

It was shown by means of IR, UV, and PMR spectra that -(3-nitro-2-pyridyl)pyruvic acid esters are practically completely enolized in the crystal state and in solution; ethyl -(3-nitro-4-pyridyl)pyruvate has an enol structure in the crystalline state and in pyridine solution but exists as a mixture of keto and enol forms in low-polarity solvents.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 389–393, March, 1974.     

Synthesis,alkylation, and molecular and crystal structure ofN-methylmorpholinium 6-amino-3,5-dicyano-1,4-dihydropyridine-4-spirocyclohexane-2-thiolate

The reaction of cyano(cyclohexylidene)thioacetamide with cyanothioacetamide or malononitrile andN-methylmorpholine yieldsN-methylmorpholinium 6-amino-3,5-dicyano-1,4-dihydropyridine-4-spirocyclohexane-2-thiolate. Its structure was established based on the results of alkylation and X-ray structural analysis.Deceased.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2535–2540, October, 1996.     

Optical waveguide sensors in analytical chemistry: today’s instrumentation, applications and trends for future development

Current concepts for chemical and biochemical sensing based on detection with optical waveguides are reviewed. The goals are to provide a framework for classifying such sensors and to assist a designer in selecting the most suitable detection techniques and waveguide arrangements. Sensor designs are categorized on the basis of the five parameters that completely describe a light wave: its amplitude, wavelength, phase, polarization state and time-dependent waveform. In the fabrication of a successful sensor, the physical or chemical property of the determined species and the particular light wave parameter to detect it should be selected with care since they jointly dictate the sensitivity, stability, selectivity and accuracy of the eventual measurement. The principle of operation, the nature or the detected optical signal, instrumental requirements for practical applications, and associated problems are analyzed for each category of sensors. Two sorts of sensors are considered: those based on direct spectroscopic detection of the analyte, and those in which the analyte is determined indirectly through use of an analyte-sensitive reagent. Key areas of recent study, useful practical applications, and trends in future development of optical waveguide chemical and biochemical sensors are considered.     

Validated ion-exclusion chromatographic method for citrate and acetate in medical fluids

In this paper we describe the development and validation of a solid-phase extraction procedure, followed by ion-exclusion chromatographic determination of citrate and acetate in medical fluids. The medical fluids contained trace levels of non-polar compounds, which were not of interest for the purposes of assay requirements, but due to their strong affinity towards the ion-exclusion chromatography column necessitated a 180-min long runtime to elute. The developed SPE procedure, based on trapping the hydrophobic compounds, on a reversed-phase material, while allowing analytes of interest elute off unretained, shortened the runtime to 35 min. The procedure is simple since it has only two steps, conditioning of the SPE cartridge with acetonitrile and treating the sample. The SPE procedure followed by ion-exclusion chromatographic determination was successfully validated per the International Conference on Harmonization (ICH) guidelines in terms of specificity, accuracy as recovery versus untreated sample, precision, range, linearity of response, ruggedness, stability of treated samples, and robustness. The validation data showed that the method is specific, accurate, precise, rugged, and robust. The validated method has been routinely used in the manufacturing environment.